CN103602945B - The method of room temperature in-situ control synthesis silver suboxide semiconductor film material - Google Patents
The method of room temperature in-situ control synthesis silver suboxide semiconductor film material Download PDFInfo
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Abstract
The present invention relates to the method for room temperature in-situ control synthesis silver suboxide semiconductor film material, it is characterized in that: surface coverage had the base material of elemental silver film to put into UV-O
3in reactor, the relative humidity keeping system is 30 ~ 90%, and under oxygen or air existent condition, 10 ~ 40 DEG C are reacted 1 ~ 2 hour, can obtain Ag in substrate surface original position
xo(AgO or Ag
2o) semiconductor film material, described UV-O
3reactor and UV-O
3cleaning machine.The method reaction process does not need to use any solvent, tensio-active agent or other chemical additive, simple to operate, less energy-consumption, and cost of manufacture is low, has wide prospects for commercial application.
Description
Technical field
The invention belongs to material chemistry technical field, particularly relate to the method for room temperature in-situ control synthesis silver suboxide semiconductor film material.
Background technology
The oxide compound of IB race argent has multiple, comprises Ag
2o, Ag
2o
3, Ag
3o
4, AgO etc., wherein Ag
2the thermal property of O is the most stable, and the critical temperature of its thermolysis is near 200-400 DEG C.It is a kind of p-type direct band-gap semicondictor material with distinct optical and electrical properties; Spectral absorption a wider range of this material, can extend to infrared region from ultraviolet region, is potential solar cell material.At present, this material all has the report be employed in light storage, magneto-optic storage, photography, detector, battery electrode etc.And AgO is a kind of compd A g of mixed valence
iag
iIIo
2with the CuO isomorphism, its thermostability is relatively weak in the oxide compound of argent, critical decomposition temperature is near 160 DEG C, but because it has potential application prospect in fields such as optoelectronic switch, intelligent glass, photothermal deformation, shieldings, this n-type semiconductor caused increasing concern in the last few years.
At present, Ag is prepared
xthe method of O semiconductor material is a lot, and conventional method has sputtering method, hot vapour deposition method, e-beam evaporation, anonizing, electrodip process, chemical deposition etc.2008, Tsutomu Shinagawa seminar delivers the article that exercise question is Direct Electrodeposition of1.46eV Bandgap Silver (I) OxideSemiconductor Films by Electrogenerated Acid on Chemistryof Materials, and this seminar adopts the AgNO of 0.20M
3with the ammoniacal liquor of 0.73M as the electrolytic solution of anode, the method for galvanic deposit is directly utilized successfully to prepare Ag at FTO conductive glass substrate surface
2o nano film material.2010, Douglas B.Chrisey seminar utilized pulsed excimer laser technology successfully to prepare Ag
2o semiconductor material, adopt the accurate laser beam of KrF to being that the silver-colored target of 4N and the solution of polysorbate 80 melt 20-80 minute containing purity, namely the throw out obtained is Ag
2o semiconductor material; They also melt by changing the Ag that the ratio of solution and kind (Polysorbate 20,40) obtain different-shape
2o material.2012, Young-Duk.Huh seminar utilized the method for precipitation to prepare Ag
2o semiconductor material, adopts the AgNO of different concns
3, pyridine and NaOH have synthesized the Ag of different-shape
2o semiconductor material.Due to the semiconductor material that AgO is a kind of mixed valence, synthesis is comparatively complicated, and it is few that the synthetic method about it is reported.1994, M.Samy El-shall seminar adopted the method for laser evaporation and control condensation to synthesize Multimetal oxide nanoparticle, comprising AgO semiconductor material at diffusion chamber.The same year, Jay A.Switzer seminar delivered the article that exercise question is Electrodeposition of Silver (II) OxideFilms on Journal of Electrochemical Society, with the sodium-acetate of 50mM Silver monoacetate and 25mM for electrolytic solution, at N
2under provide protection, current density is controlled at 0.25mA/cm
2successfully go out AgO semiconductor material at substrates of the stainless steel-based end.Although adopt these methods all successfully to prepare Ag
xo semiconductor material, but consider the high temperature required by these methods, high pressure, high vacuum, the severe condition such as electric field, atmosphere protection or high energy consumption, and the equipment that reaction process needs is complicated, and the product synthesized is Ag substantially
xo powder, needs the deficiencies such as further film forming in the preparation process of subsequent device.
Based on Ag
xthe excellent physical properties that O thin-film material is numerous and good prospects for commercial application, study a kind of less energy-consumption, be swift in response, production cost is low, the preparation Ag of environmental protection
xthe method of O semiconductor film material will be of great significance by tool, and can meet the requirement of current social to energy-saving and emission-reduction well.
Summary of the invention
Technical problem to be solved by this invention be for prepare at present exist in silver suboxide semiconductor material preparation process dependence electric field, high vacuum, high energy consumption, reaction process is complicated and can only generate the shortcomings such as powder, a kind of room temperature in-situ control is provided to synthesize the method for silver suboxide semiconductor film material, the method reaction process does not need to use any solvent, tensio-active agent or other chemical additive, simple to operate, less energy-consumption, cost of manufacture is low, has wide prospects for commercial application.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The method of room temperature in-situ control synthesis silver suboxide semiconductor film material, is characterized in that: surface coverage had the base material of elemental silver film to put into UV-O
3reactor and UV-O
3in cleaning machine (UV ozone cleaning machine), the relative humidity keeping system is 30 ~ 90%, and under oxygen or air existent condition, 10 ~ 40 DEG C are reacted 1 ~ 2 hour, can obtain Ag in substrate surface original position
xo(AgO or Ag
2o) semiconductor film material.
In such scheme, the thickness of described elemental silver film is 60-100nm.
In such scheme, the film of the elemental silver forming thin film of described substrate material surface is magnetically controlled DC sputtering, plating or hot evaporation.
In such scheme, described UV-O
3reactor and UV-O
3in cleaning machine (UV ozone cleaning machine), UV lamp luminescence power is 20-30mW/cm
2, surface coverage has the distance of the base material of elemental silver film and UV fluorescent tube to remain on 6.0-10.0cm.
In such scheme, described base material is not oxidizable material, includes but not limited to ITO conductive glass or mat glass.
In such scheme, described UV-O
3reactor and UV-O
3the commercially available acquisition of cleaning machine, it can use NavascanTechnologies, the UV-O of the PSD-UV4 model of Inc. manufacturer production
3the UV-O of the PSD-UV8 model of cleaning machine or Navascan Technologies, Inc. manufacturer production
3cleaning machine, but be not limited to this.
In such scheme, when described reaction is carried out, can by UV-O
3reactor and UV-O
3inlet mouth (air inlet port) and air outlet (production well) of cleaning machine seal.So to avoid O
3shed to the harm of environment.
In such scheme, when described reaction is carried out under oxygen existence condition, can by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, then by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine and air outlet seal reacts.
Advantage of the present invention:
1, room temperature reaction, mild condition, on conductive substrates such as oxide compounds without impact, reaction process is controlled, easy to operate, and reaction required time is short, and energy consumption is low, is conducive to low cost scale operation and makes Ag
xo semiconductor film material, has good laboratory and prepares in enormous quantities and industrial scale prospect of production.
2, technique is simple, at substrate surface direct formation of film at surface, can not need aftertreatment, overcomes the shortcomings such as the high vacuum of the preparation methods such as high vacuum thermal evaporation reaction, pulse laser film forming, electrochemical filming, high energy consumption, reaction and film process complexity.
3, prepared film macroscopic view geometrical shape is controlled, utilizes mask to control the geometrical shape of sputtering or hot evaporation elemental silver film, can realize product A g
xthe control of O semiconductor film macroscopic view geometrical shape.
4, by controlling the condition such as thin film-forming method, elemental silver film thickness, reaction times, temperature, relative humidity and different base, can control Ag well
xthe kind of O semiconductor film material, pattern, size, thickness, crystalline phase and dominant growth crystal face etc.
Accompanying drawing explanation
The scanning electron photomicrograph of the AgO semiconductor optoelectronic thin-film material of Fig. 1, embodiment 1 preparation
The XRD figure spectrum of the AgO semiconductor optoelectronic thin-film material of Fig. 2, embodiment 1 preparation
The scanning electron photomicrograph of the AgO semiconductor optoelectronic thin-film material of Fig. 3, embodiment 2 preparation
The XRD figure spectrum of the AgO semiconductor optoelectronic thin-film material of Fig. 4, embodiment 2 preparation
The scanning electron photomicrograph of the AgO semiconductor optoelectronic thin-film material of Fig. 5, embodiment 3 preparation
The XRD figure spectrum of the AgO semiconductor optoelectronic thin-film material of Fig. 6, embodiment 3 preparation
The ultraviolet-visible absorption spectroscopy collection of illustrative plates of the AgO semiconductor optoelectronic thin-film material of Fig. 7, embodiment 3 preparation
The scanning electron photomicrograph of the AgO semiconductor optoelectronic thin-film material of Fig. 8, embodiment 4 preparation
The XRD figure spectrum of the AgO semiconductor optoelectronic thin-film material of Fig. 9, embodiment 4 preparation
The scanning electron photomicrograph of the AgO semiconductor optoelectronic thin-film material of Figure 10, embodiment 5 preparation
The XRD figure spectrum of the AgO semiconductor optoelectronic thin-film material of Figure 11, embodiment 5 preparation
The Ag of Figure 12, embodiment 6 preparation
2the scanning electron photomicrograph of O semiconductor optoelectronic thin-film material
The Ag of Figure 13, embodiment 6 preparation
2the XRD figure spectrum of O semiconductor optoelectronic thin-film material
The Ag of Figure 14, embodiment 6 preparation
2the ultravioletvisible absorption light collection of illustrative plates of O semiconductor optoelectronic thin-film material
The Ag of Figure 15, embodiment 7 preparation
2the scanning electron photomicrograph of O semiconductor optoelectronic thin-film material
The Ag of Figure 16, embodiment 7 preparation
2the XRD figure spectrum of O semiconductor optoelectronic thin-film material
The Ag of Figure 17, embodiment 8 preparation
2the scanning electron photomicrograph of O semiconductor optoelectronic thin-film material
The Ag of Figure 18, embodiment 8 preparation
2the XRD figure spectrum of O semiconductor optoelectronic thin-film material
The Ag of Figure 19, embodiment 9 preparation
2the scanning electron photomicrograph of O semiconductor optoelectronic thin-film material
The Ag of Figure 20, embodiment 9 preparation
2the XRD figure spectrum of O semiconductor optoelectronic thin-film material
Embodiment:
Summary of the invention of the present invention is further illustrated below by embodiment.
Embodiment 1:
1, preparation work: ITO conductive glass is used successively liquid detergent, deionized water ultrasonic cleaning 20min, then the mixing solutions 80 DEG C process 30min of strong aqua (mass percent 25%)/hydrogen peroxide (mass percent 30%)/deionized water (volume ratio is 1:2:5) is used, finally use deionized water ultrasonic cleaning 20min, the ITO conductive glass handled well is dry under 80 DEG C of conditions, is kept in clean moisture eliminator stand-by.Utilize DC magnetron sputtering method to sputter the elemental silver thin film layer that a layer thickness is 60nm in the substrate of ITO conductive glass, control silver thickness with film thickness monitoring (FTM), the ITO conductive glass that gained has elemental silver thin film layer is kept in moisture eliminator stand-by.
2, reactions steps: control reaction conditions and temperature remain on 10 DEG C, and relative humidity remains on 30%, and the ITO conductive glass with elemental silver thin-film surface is directly put into UV-O
3in reactor, pass into oxygen by inlet mouth, then UV-O
3inlet mouth and the air outlet of reactor seal.React and take out sample after 1 hour, products therefrom is taupe film.The ITO conductive glass that gained has a silver oxide film is put into moisture eliminator preserve.Described UV-O
3reactor and UV-O
3cleaning machine is the UV-O of the PSD-UV4 model of Novascan Technologies, Inc. manufacturer production
3cleaning machine (UV ozone cleaning machine), wherein UV lamp luminescence power is 20-30mW/cm
2namely the interior energy consumed of the area of every square centimeter of fluorescent tube is 20-30mW, and surface coverage has the ITO conductive glass of elemental silver film and the distance of UV fluorescent tube to remain on 8.0cm.Fig. 1 is the SEM photo of gained sample.Fig. 2 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for AgO semiconductor film material, (200), (002) in figure, (111), (-202), (-311) are all diffraction peaks of the different crystal face of AgO.
Embodiment 2:
1, preparation work: adopt and the method identical with embodiment 1, the substrate of ITO conductive glass sputters the elemental silver thin film layer that thickness is 100nm.
2, reactions steps: control reaction conditions and temperature remain on 22 DEG C, and relative humidity remains on 40%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O above-mentioned surface coverage
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into 5L oxygen, then UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 80min, products therefrom is taupe film.The ITO conductive glass that gained has a silver oxide film is put into moisture eliminator preserve.Fig. 3 is the SEM photo of gained sample.Fig. 4 is the XRD figure of gained sample, characterize through XRD and obtain: the present embodiment gained for AgO semiconductor film material, (200), (002) in figure, (111), (-202), (-311) are all diffraction peaks of the different crystal face of AgO, another compared with embodiment 1, the relative intensity of diffraction peak (200), (111) crystal face comparatively embodiment 1 strengthens to some extent.
Embodiment 3:
1, preparation work: adopt the method identical with embodiment 1, the substrate of ITO conductive glass sputters the elemental silver thin film layer that thickness is 100nm.
2, reactions steps: control reaction conditions and temperature remain on 22 DEG C, and relative humidity remains on 50%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O above-mentioned surface coverage
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen in reactor, then the inlet mouth of reactor and air outlet is sealed, and take out sample after reaction 80min, products therefrom is taupe film.The ITO conductive glass that gained has a silver oxide film is put into moisture eliminator preserve.Fig. 5 is the SEM photo of gained sample.Fig. 6 is the XRD figure of gained sample, characterize through XRD and obtain: the present embodiment gained for AgO semiconductor film material, separately as seen from the figure, along with the increase of temperature of reaction and system relative humidity, the diffraction peak (200) of AgO, the relative intensity of (111) crystal face comparatively embodiment 1 obviously strengthen.Fig. 7 is the ultraviolet-visible absorption spectroscopy figure of gained sample, and as seen from the figure, AgO nanometer particle film all has absorption in visible region and near-infrared region.
Embodiment 4:
1, preparation work: adopt the method identical with embodiment 1, the substrate of ITO conductive glass sputters the elemental silver thin film layer that thickness is 100nm.
2, reactions steps: control reaction conditions and temperature remain on 22 DEG C, and relative humidity remains on 60%, surface coverage is had the ITO conductive glass of the elemental silver thin film layer of one deck 100nm directly put into UV-O
3reactor and UV-O
3in cleaning machine, take out sample after directly utilizing air reaction 1h, products therefrom is taupe film.The ITO conductive glass that gained has a silver oxide film is put into moisture eliminator preserve.Fig. 8 is the SEM photo of gained sample.Fig. 9 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for AgO semiconductor film material, (200), (002) in figure, (111), (-202), (-311) are all diffraction peaks of the different crystal face of AgO.Another as seen from the figure, along with the diffraction peak (200) of the increase AgO of temperature and system relative humidity, (111) crystal face relative intensity comparatively embodiment 1 also obviously strengthen.Same Fig. 7 of ultraviolet-visible absorption spectroscopy figure of gained sample.
Embodiment 5:
1, preparation work: mat glass is used successively liquid detergent, deionized water ultrasonic cleaning 20min, then the mixing solutions 80 DEG C process 30min of strong aqua (mass percent 25%)/hydrogen peroxide (mass percent 30%)/deionized water (volume ratio is 1:2:5) is used, finally use deionized water ultrasonic cleaning 20min, the mat glass handled well is dry under 80 DEG C of conditions, is kept in clean moisture eliminator stand-by.Utilize DC magnetron sputtering method in mat glass substrate, sputter the elemental silver thin film layer that thickness is 100nm, control silver thickness with film thickness monitoring (FTM), the mat glass that gained has elemental silver thin film layer is kept in moisture eliminator stand-by.
2, reactions steps: control reaction conditions and temperature remain on 22 DEG C, and relative humidity remains between 50-60%, has the mat glass of elemental silver thin film layer directly to put into UV-O surface sputtering
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 1h, products therefrom is taupe film.The mat glass that gained has a silver oxide film is put into moisture eliminator preserve.Figure 10 is the SEM photo of gained sample.Figure 11 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for AgO semiconductor film material, (200), (002) in figure, (111), (-202), (-311) are all diffraction peaks of the different crystal face of AgO.
Embodiment 6:
1, preparation work: utilize DC magnetron sputtering method to sputter the elemental silver thin film layer that a layer thickness is 60nm in the substrate of ITO conductive glass.
2, reactions steps: control reaction conditions and temperature remain on 32 DEG C, and relative humidity remains on 60%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O above-mentioned surface sputtering
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 1h, products therefrom is taupe film, the ITO conductive glass that gained has a silver oxide film is put into moisture eliminator and preserves.Figure 12 is the SEM photo of gained sample.Figure 13 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for Ag
2o semiconductor film material, in figure, (111), (200), (220) are all Ag
2the diffraction peak of the different crystal face of O.Figure 14 is the ultraviolet-visible absorption spectroscopy figure of gained sample, as seen from the figure: Ag
2o nanometer particle film is in ultraviolet, and all there is absorption visible region and near-infrared region.
Embodiment 7:
1, preparation work: the method adopting same embodiment 1, the substrate of ITO conductive glass sputters the elemental silver thin film layer that thickness is 100nm.
2, reactions steps: control reaction conditions and temperature remain on 28 DEG C, and relative humidity remains on 70%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O above-mentioned surface sputtering
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 80min, products therefrom is taupe film, the ITO conductive glass that gained has a silver oxide film is put into moisture eliminator and preserves.Figure 15 is the SEM photo of gained sample.Figure 16 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for Ag
2o semiconductor film material, in figure, (111), (200), (220) are all Ag
2the diffraction peak of the different crystal face of O, the relative intensity of diffraction peak (200) crystal face comparatively embodiment 6 obviously strengthens.Same Figure 14 of ultraviolet-visible absorption spectroscopy figure of gained sample.
Embodiment 8:
1, preparation work: the method adopting same embodiment 1, the substrate of ITO conductive glass sputters the elemental silver thin film layer that thickness is 60nm.
2, reactions steps: control reaction conditions and temperature remain on 25 DEG C, and relative humidity remains on 90%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O sputtering
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 80min, products therefrom is taupe film, the ITO conductive glass that gained has a silver oxide film is put into moisture eliminator and preserves.Figure 17 is the SEM photo of gained sample.Figure 18 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for Ag
2o semiconductor film material, in figure, (111), (200), (220) are all Ag
2the diffraction peak of the different crystal face of O, the relative intensity of diffraction peak (111) crystal face comparatively embodiment 7 obviously strengthens, and the relative intensity of (200) crystal face obviously weakens.
Embodiment 9:
1, preparation work: ITO conductive glass is used successively liquid detergent, deionized water ultrasonic cleaning 20min, then the mixing solutions 80 DEG C process 30min of strong aqua (mass percent 25%)/hydrogen peroxide (mass percent 30%)/deionized water (volume ratio is 1:2:5) is used, finally use deionized water ultrasonic cleaning 20min, the ITO conductive glass handled well is dry under 80 DEG C of conditions, is kept in clean moisture eliminator stand-by.Utilize hot evaporation to steam the filamentary silver of 40cm, the ITO conductive glass that gained has elemental silver thin film layer is kept in moisture eliminator stand-by.
2, reactions steps: control reaction conditions and temperature remain on 35 DEG C, and relative humidity remains on 70%, has the ITO conductive glass of elemental silver thin film layer directly to put into UV-O above-mentioned hot evaporation
3reactor and UV-O
3in cleaning machine, by UV-O
3reactor and UV-O
3the inlet mouth of cleaning machine passes into oxygen, UV-O in reactor
3inlet mouth and the air outlet of reactor seal.Take out sample after reaction 80min, products therefrom is taupe film, the ITO conductive glass that gained has a silver oxide film is put into moisture eliminator and preserves.Figure 19 is the SEM photo of gained sample.Figure 20 is the XRD figure of gained sample, characterizes obtain through XRD: the present embodiment gained for Ag
2o semiconductor film material, in figure, (111), (200) are all Ag
2the diffraction peak of the different crystal face of O, the relative intensity of diffraction peak (200) crystal face comparatively embodiment 7 obviously strengthens.
Claims (5)
1. the method for room temperature in-situ control synthesis silver suboxide semiconductor film material, is characterized in that: surface coverage had the base material of elemental silver film to put into UV-O
3in reactor, the relative humidity keeping system is 30 ~ 90%, under oxygen or air existent condition, and 10 ~ 40
0c reaction 1 ~ 2 hour, can obtain Ag in substrate surface original position
xo semiconductor film material, described UV-O
3reactor and UV-O
3cleaning machine, described Ag
xo is AgO or Ag
2o.
2. the method for room temperature in-situ control synthesis silver suboxide semiconductor film material according to claim 1, is characterized in that: the thickness of described elemental silver film is 60-100nm.
3. the method for room temperature in-situ control synthesis silver suboxide semiconductor film material according to claim 1, is characterized in that: the film of the elemental silver forming thin film of described substrate material surface is magnetically controlled DC sputtering, plating or hot evaporation.
4. the method for room temperature in-situ control synthesis silver suboxide semiconductor film material according to claim 1, is characterized in that: described UV-O
3in cleaning machine, UV lamp luminescence power is 20-30mW/cm
2, surface coverage has the distance of the base material of elemental silver film and UV fluorescent tube to remain on 6.0-10.0cm.
5. the method for room temperature in-situ control synthesis silver suboxide semiconductor film material according to claim 1, is characterized in that: described base material is not oxidizable material.
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